CN111342128B - Formation method of low-temperature lithium ion battery - Google Patents
Formation method of low-temperature lithium ion battery Download PDFInfo
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- CN111342128B CN111342128B CN202010099386.1A CN202010099386A CN111342128B CN 111342128 B CN111342128 B CN 111342128B CN 202010099386 A CN202010099386 A CN 202010099386A CN 111342128 B CN111342128 B CN 111342128B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a formation method of a low-temperature lithium ion battery, wherein an electrolyte of the lithium ion battery contains an organic solvent and an additive, the organic solvent consists of DMC and EC, the additive comprises N, N-dimethyl trifluoroacetamide and vinylene carbonate, and the volume ratio of the N, N-dimethyl trifluoroacetamide to the vinylene carbonate is 1: 3.5-3.7; the invention relates to a method for preparing a special electrolyte and an additive, which aims at the special electrolyte and the additive, and pulse charge-discharge circulation is carried out between a first preset voltage and a second preset voltage at low temperature, so that the low-temperature circulation performance of the battery is improved.
Description
Technical Field
The invention relates to a formation method of a low-temperature lithium ion battery.
Background
In the lithium ion battery, the conductivity is reduced due to the increase of the viscosity of the electrolyte at low temperature, so that the rate performance is affected, and the battery cannot exert the original capacity at low temperature due to the polarization of the electrode inside the battery. The invention provides a formation method of a low-temperature lithium ion battery, and the battery subjected to the formation method can still exert normal capacity after the working temperature is recovered to be normal.
Disclosure of Invention
The invention provides a formation method of a low-temperature lithium ion battery, wherein an electrolyte of the lithium ion battery contains an organic solvent and an additive, the organic solvent consists of DMC and EC, the additive comprises N, N-dimethyl trifluoroacetamide and vinylene carbonate, and the volume ratio of the N, N-dimethyl trifluoroacetamide to the vinylene carbonate is 1: 3.5-3.7; the invention relates to a method for preparing a special electrolyte and an additive, which aims at the special electrolyte and the additive, and pulse charge-discharge circulation is carried out between a first preset voltage and a second preset voltage at low temperature, so that the low-temperature circulation performance of the battery is improved.
The specific scheme is as follows:
a chemical synthesis method of a low-temperature lithium ion battery comprises an electrolyte of the lithium ion battery, wherein the electrolyte of the lithium ion battery comprises an organic solvent and an additive, the organic solvent consists of DMC and EC, the additive comprises N, N-dimethyl trifluoroacetamide and vinylene carbonate, and the volume ratio of the N, N-dimethyl trifluoroacetamide to the vinylene carbonate is 1: 3.5-3.7; the formation method comprises the following steps:
1) injecting electrolyte, standing, vacuumizing and sealing;
2) charging to a first preset voltage by constant current;
3) reducing the temperature of the battery to below zero ℃;
4) performing constant current pulse charge-discharge circulation between a first preset voltage and a second preset voltage;
5) charging at a second predetermined voltage;
6) adjusting the temperature of the battery to normal temperature, and charging the battery at constant current to a charging cut-off voltage;
7) charging at constant voltage with a charge cut-off voltage, and standing;
8) and carrying out constant-current charge-discharge circulation for several times between the charge cut-off voltage and the discharge cut-off voltage.
Further, wherein the first predetermined voltage is 3.05-3.10V; the second predetermined voltage is 3.15-3.20V.
Further, the charging current in the step 2 is 0.01-0.02C.
Further, in the step 3, the temperature of the battery is adjusted to-10-0 ℃.
Further, the volume ratio of DMC and EC in the organic solvent is 3: 1.
Further, the content of the N, N-dimethyl trifluoroacetamide is 1 to 1.5 volume percent, and the content of the vinylene carbonate is 3.5 to 5 volume percent.
Further, the step 4 pulse charge-discharge cycle comprises charging to a second predetermined voltage with a current pulse of 0.02-0.05C, and discharging to a first predetermined voltage with a current pulse of 0.02-0.05C, wherein the pulse time is 10-30s, and the interval is 1-3 s.
The invention has the following beneficial effects:
1) the inventor finds that the low-temperature performance of the battery can be greatly improved by adding N, N-dimethyl trifluoroacetamide and vinylene carbonate together in specific content, and the performance attenuation of the battery after low-temperature operation is low.
2) And DMC and EC with excellent low-temperature performance are selected as solvents in the electrolyte, and the low-temperature conductivity is improved by matching with additives in a specific concentration range.
3) And pulse charge-discharge circulation is carried out in a specific voltage range interval aiming at a specific electrolyte system to form a stable SEI film, so that the method has a great promotion effect on recovering the battery capacity.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
The active material of the positive electrode is provided as LiCoO2(ii) a The electrolyte comprises 1M lithium hexafluorophosphate, DMC + EC in a volume ratio of 3:1, N-dimethyl trifluoroacetamide and vinylene carbonate as additives, wherein the content of the N, N-dimethyl trifluoroacetamide is 1-1.5 volume percent, and the content of the vinylene carbonate is 3.5-5 volume percent; the active material of the negative electrode was an artificial graphite negative electrode, and the charge cut-off voltage was 2.7V and the discharge cut-off voltage was 4.2V.
Example 1
1) Injecting electrolyte, standing for 1h, vacuumizing and sealing, wherein the content of the N, N-dimethyl trifluoroacetamide in the electrolyte is 1 volume percent, and the content of the vinylene carbonate is 3.5 volume percent;
2) charging to a first preset voltage at a constant current of 0.01C, wherein the first preset voltage is 3.05V;
3) reducing the temperature of the battery to-10 ℃;
4) performing a constant current pulse charge-discharge cycle between a first predetermined voltage and a second predetermined voltage, wherein the second predetermined voltage is 3.15V, the pulse charge-discharge cycle comprises charging to the second predetermined voltage with a current pulse of 0.02C, and then discharging to the first predetermined voltage with a current pulse of 0.02C, wherein the pulse time is 30s, and the interval is 3 s;
5) charging at a second preset voltage and constant voltage until the charging current is less than 0.01C;
6) adjusting the temperature of the battery to normal temperature, and charging the battery to a charging cut-off voltage at a constant current of 0.05 ℃;
7) charging at constant voltage with a charge cut-off voltage until the charging current is less than 0.01C, and standing for 1 h;
8) the charge and discharge were cycled between the charge cutoff voltage and the discharge cutoff voltage at a constant current of 0.05C for 4 cycles.
Example 2
1) Injecting electrolyte, standing for 1h, vacuumizing and sealing, wherein the content of the N, N-dimethyl trifluoroacetamide in the electrolyte is 1.5 volume percent, and the content of the vinylene carbonate is 5 volume percent;
2) charging to a first preset voltage at a constant current of 0.02C, wherein the first preset voltage is 3.10V;
3) reducing the temperature of the battery to 0 ℃;
4) performing a constant current pulse charge-discharge cycle between a first predetermined voltage and a second predetermined voltage, wherein the second predetermined voltage is 3.20V, the pulse charge-discharge cycle comprises charging to the second predetermined voltage with a current pulse of 0.05C, and then discharging to the first predetermined voltage with a current pulse of 0.05C, the pulse time is 10s, and the interval is 1 s;
5) charging at a second preset voltage and constant voltage until the charging current is less than 0.01C;
6) adjusting the temperature of the battery to normal temperature, and charging the battery to a charging cut-off voltage at a constant current of 0.2 ℃;
7) charging at constant voltage with a charge cut-off voltage until the charging current is less than 0.01C, and standing for 1 h;
8) the charge and discharge were cycled 4 times at a constant current of 0.2C between the charge cutoff voltage and the discharge cutoff voltage.
Example 3
1) Injecting electrolyte, standing for 1h, vacuumizing and sealing, wherein the content of the N, N-dimethyl trifluoroacetamide in the electrolyte is 1.2 volume percent, and the content of the vinylene carbonate is 4.3 volume percent;
2) charging to a first preset voltage at a constant current of 0.01C, wherein the first preset voltage is 3.08V;
3) reducing the temperature of the battery to-5 ℃;
4) performing a constant current pulse charge-discharge cycle between a first predetermined voltage and a second predetermined voltage, wherein the second predetermined voltage is 3.18V, the pulse charge-discharge cycle comprises charging to the second predetermined voltage with a current pulse of 0.03C, and then discharging to the first predetermined voltage with a current pulse of 0.03C, wherein the pulse time is 20s, and the interval is 2 s;
5) charging at a second preset voltage and constant voltage until the charging current is less than 0.01C;
6) adjusting the temperature of the battery to normal temperature, and charging the battery to a charging cut-off voltage at a constant current of 0.1 ℃;
7) charging at constant voltage with a charge cut-off voltage until the charging current is less than 0.01C, and standing for 1 h;
8) the charge and discharge were cycled 4 times at a constant current of 0.1C between the charge cutoff voltage and the discharge cutoff voltage.
Comparative example 1
1) Injecting electrolyte, standing for 1h, vacuumizing and sealing, wherein the content of the N, N-dimethyl trifluoroacetamide in the electrolyte is 1.2 volume percent, and the content of the vinylene carbonate is 4.3 volume percent;
2) charging to a charge cut-off voltage at a constant current of 0.1C;
3) charging at constant voltage with a charge cut-off voltage until the charging current is less than 0.01C, and standing for 1 h;
4) the charge and discharge were cycled 4 times at a constant current of 0.1C between the charge cutoff voltage and the discharge cutoff voltage.
Comparative example 2
The electrolyte only contains N, N-dimethyl trifluoroacetamide as an additive, the content of the N, N-dimethyl trifluoroacetamide is 1.2 volume percent, and other technological parameters are the same as those in example 3.
Comparative example 3
The electrolyte contained vinylene carbonate as an additive only, and its content was 4.3 vol%, and the other processes were the same as in example 3.
Comparative example 4
The content of N, N-dimethyltrifluoroacetamide in the electrolyte was 1.2 vol%, the content of vinylene carbonate was 2 vol%, and the other processes were the same as in example 3.
Experiment and data
The batteries obtained according to the formation methods of examples 1 to 3 and comparative examples 1 to 4 were subjected to charge-discharge cycles 100 times at-10 ℃ to test the capacity retention rate, and then the battery temperature was returned to room temperature to measure the capacity retention rate, and the results are shown in the following table. The combination of the two additives has high capacity retention rate at low temperature, can improve the low-temperature capacity retention rate within a specific content range, and is pulsed at a specific voltage to help improve the recovery capability of the battery capacity at normal temperature.
TABLE 1
| Low temperature (%) | Room temperature (%) | |
| Example 1 | 88.9 | 96.9 |
| Example 2 | 89.1 | 97.2 |
| Example 3 | 89.6 | 97.8 |
| Comparative example 1 | 88.4 | 92.3 |
| Comparative example 2 | 85.1 | 90.2 |
| Comparative example 3 | 76.9 | 84.5 |
| Comparative example 4 | 82.4 | 88.9 |
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (5)
1. A chemical synthesis method of a low-temperature lithium ion battery comprises an electrolyte of the lithium ion battery, wherein the electrolyte of the lithium ion battery comprises an organic solvent and an additive, the organic solvent consists of DMC and EC, the additive comprises N, N-dimethyl trifluoroacetamide and vinylene carbonate, the content of the N, N-dimethyl trifluoroacetamide is 1-1.5% by volume, and the content of the vinylene carbonate is 3.5-5% by volume; the volume ratio of the N, N-dimethyl trifluoroacetamide to the vinylene carbonate is 1: 3.5-3.7; the formation method comprises the following steps:
1) injecting electrolyte, standing, vacuumizing and sealing;
2) charging to a first preset voltage by constant current; wherein the first predetermined voltage is 3.05-3.10V;
3) reducing the temperature of the battery to below zero ℃;
4) performing constant current pulse charge-discharge circulation between a first preset voltage and a second preset voltage; the second preset voltage is 3.15-3.20V;
5) charging at a second predetermined voltage;
6) adjusting the temperature of the battery to normal temperature, and charging the battery at constant current to a charging cut-off voltage;
7) charging at constant voltage with a charge cut-off voltage, and standing;
8) and carrying out constant-current charge-discharge circulation for several times between the charge cut-off voltage and the discharge cut-off voltage.
2. The chemical conversion method according to claim 1, wherein the charging current in step 2 is 0.01-0.02C.
3. The method according to claim 1, wherein in the step 3, the temperature of the battery is adjusted to-10 to 0 ℃.
4. The method of claim 1, wherein the volume ratio of DMC to EC in the organic solvent is 3: 1.
5. The method of claim 1, wherein said step 4 pulse charge and discharge cycle comprises charging to a second predetermined voltage with a current pulse of 0.02-0.05C and discharging to a first predetermined voltage with a current pulse of 0.02-0.05C, said pulses having a time of 10-30s with an interval of 1-3 s.
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| CN112201870B (en) * | 2020-10-22 | 2022-10-11 | 苏州极闪控电信息技术有限公司 | Multi-section formation method of lithium ion battery |
| CN114497777B (en) * | 2022-01-10 | 2024-02-13 | 清华大学 | Method for forming lithium ion battery and lithium ion battery |
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Effective date of registration: 20210806 Address after: 344000 houfa Industrial Park, Le'an County, Fuzhou City, Jiangxi Province Applicant after: JIANGXI JINHUI LITHIUM BATTERY MATERIAL Co.,Ltd. Address before: 215000 room 404, building 8, century garden, Huqiu District, Suzhou City, Jiangsu Province Applicant before: Qian Qi |
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